Process of making pectous material and product



. Patented 26, 1935 mocass or Mame PECTOUS MATERIAL ANnrnonUc'r Herbert 1 La,- Clarence 0. Taylor, in Frederick A. Beck,'Anahel m, Call No Drawing. Application October 16, 193

' Serial No. 693,892 a This invention relates to a process of making pectous material and to the product thereby produced. More particularly, the invention relates to the preparationof a dry, standardized mixture of finely divided fibrous material containing pectose in substantially its original state and a filter aid, such as diatomaceous earth.

it has previously been suggested (Beyli'k Patent No. 1,393,660) that a dry, fibrous material containing pectose uniformly distributed throughout the cells of the fiber, could be obtained by dissolving from comminute'd fruit pulp and the like.

' the alcohol soluble constituents of the fruit pulp.

Such a process, however, has the disadvantage that it is relatively expensive, as compared with our'present process, and also that'it does not remove a number or water-soluble substances as completely as isdesirable.

According to our present process, the watersoluble ingredients of fruit pulp are removed by simply washing and extracting with water and then pressing the extracted mass with the help of a filter aid under considerable pressure. The product so produced comprising a mixture of fibrous vegetable tissues containing the original pectose content, and'the filter aid, is then standardized to a definite jell strength and may be used "temperatures as are readily available, in order to in the making of jellies and the like by subjecting the mixture to an acid digestive treatment. This is necessary, since the pectous material in the dry standardized product is in a water insoluble form and must be first hydrolyzed by means of an acid digestive step in order to render the pectous material available for jelly making purposes.

It is therefore an object of this invention to provide a relatively economical and simple method for .the preparation 01 a dry,,standardized pectous product containing fibrous material with the original pectose-content distributed therein, and a filter aid to assist in the subsequent extraction or the available pectin content upon acid digestion of the mixture.

It is a further important object of this invention to provide a dry, standardized pectous material v having an insoluble pectose content thatmay .be

renderedasily available by digestion otthe materialwith an acid.

and drying, it is impossible to prevent enzymic 5 Claims. (01:99-11) Various. pectose bearing fruit and vegetable materials may be used as the raw material for making our product. Oranges, lemons, limes and I grapefruits all contain large quantities of pectose,

themother substance that yields pectinupon hy- 5 drolysis. In addition'to these citrus fruits, our 1 invention also includes the use of apples, or apple pomace, as a source oi. pectose.

Heretofore pectin has been obtained from these citrus fruits and apples by extracting the fruit pulp with an aqueous acid solution to effect hydrolysis of the pectose. After hydrolysis, the 'digested fruit pulp had been subjected to filtration and the pectin content of the filtrate had been precipitated with either aluminum hydroxide orwith alcohol, and subsequently purified. These steps have all been necessary in order. to avoid contaminating the finalproduct with the very strong flavors, and especially the. bitter oils that always appear in citrus fruits.

. According to our present process, the citrus fruit or apple pomace, or other source of pectose, is pressed to remove the juicesandalso the oils. The mass is then ground very fine and washed repeatedly with water at the usual tap temperatures in any convenient apparatus. This washing process should be done rapidly and at as low avoid fermentation'due to enzymic action.

The vdiatomaceous earth is then added in sufilcient quantity to assistin the filtration and pressing of the pulp mass-to remove as much as possible of the liquid content. By diatoinaceous earth' is meant any 01' the various forms oi iniusorial earth,

kieselguhr and the like that are' commonly used as filter aids' and sold under various trademarks, such as Hypocel.

The amount of diatomaceous earth used may vary from one pound to ten pounds for each ten gallons of drained, water-washed fruit pulp. The 40 variation in the quantity of diatqmaceous earth takes into account the texture and conditionof the fruit. when slimy, and hard to press, more diatomaceous earth is necessary.

Inasmuch as alkaline conditions are harmifulf to pectous materials, it may be necessary at this stagefto add a slight acidity tothe peel, or fruit pulp. We ha'vealso foimd that enzymes destroy and digest citrus peels very readily, so that to prevent this, it is desirable, but not absolutely necessary, to add sulphurous acid, either added as suchofr formed by'the action oi'-sulphur dioxide on the water presentin the mass. when a long period of time elapses between pressing action without taking some such positive as as this. i

The wet pulpy mass, with the earth material admixed therewith, is now run into a press and pressed out thoroughly. Great pressure may be exerted with the earth material present and a larger proportion of liquid content may theremay be employed, but we prefer to use a rotary drier with heated air and to use a steam jacketed or otherwise heated shell.

The dried material contains varying amounts of diatomaceous earth and also, depending upon the raw material used, varying proportions of pectose. In order to establish the pectin value of the product, and standardize it for jelly strength, we use the following method:

For instance, grams of the dry fibrous material is admixed with 1000 cc. water, the mass brought to a boil and an acid, preferably hydrochloric, added. The added hydrochloric acid,

together with any fruit acidm'esent or added thereto, should be suificient to bring the pH value within the relatively narrow range of 2.40 to 2.65. A lower pH value is conducive of producing too much pectic acid and a pH above 2.65

will not extract pectin eificiently.

The acidified mass is heated for half an hour at boiling temperature orti'iereabouts and then pressed out'in a small'fruit bag press. Since the hot pectin liquor is too strongly acid for jelly making, the acidity is partially. neutralized by the addition of about 6 cc. of sodium acetate solution containing 1 gram of sodiumacetate-to; each 11 cc. of solution, based upon '1000 cc. of.

extract. I 350 cc. of the partially neutralizedextract is then measured out and 500 grams of sugar (ordinary cane sugar) are added thereto. The result-.- ing mass is boiled down to a welsht of exactly 770 grams and poured into 8 ounce tumblers, to which have previously been added 4 cc. of 50% citric acid solution. .The liquid in the tumblers is stirred quickly and then allowed to stand.

Jelly will form immediately.

11 the-jelly is too weak alter standing 12 hours,

increasing amounts of extract with 500 grams of sugar are tried out, always boiling the liquid mass to exactly 770 grams before pourlngzinto the tumblers. When theriuht' texture of ielly is reached, as determined by the usual jelly makers "test, the grade of peel, or fruit pulp, is vfigured as'followsz- Amount of liquid for jelly snaking SEQ Total extract from peel X where x is the number of grains of sugar the total amount of extract will Jell. Consequently,

;Grade of the Number of grams of fruit'peel, or peel pulp, cooked In order to standardize the peel to some predetermined strength, either pectous material of higher and known strength is mixed therewith,

- tracting the pectin formed as a result of the 5 hydrolysis of pectose according to an acid digestion treatment, such as above described, The actual extraction of-the pectin solution may be best eifected ina type of press, such as described in the application of Herbert T. Leo above referred to. If the conditions outlined above for extraction oi the pectin be followed, such as the use of a pH range between 2.40 and 2.65, time of boiling, etc., a. liquid pectin solution of known Jell strength and of predetermined pH value will 15 be obtained. This pectin solution may be used directlyin the manufacture of jellies and the like, or for other purposes for which pectin is usually employed.

It will be noted that the diatomaceous earth 20 serves not only as a filter aid in the filtering and pressing of the fruit pulp or pomace, but also in the extraction of the available pectin content from the dry, powdered fibrous material of our standardized product. The diatomaceous 5 earth also serves in the extraction of the oils and flavor from the fruit peel or pomace by absorbing and retaining a certain amount of such oils and flavors, thereby making it possible to remove the bitter oils from citrus fruits without 30 the use of organic solvents. In addition-to these functions, the diatomaceous earth also serves in the final product as a diluent, by means of which the product may be standardized to a definite jell strength,

In order to obtain uniform results, it is important to follow the conditions specified for the standardizationof our product, These conditions include the following:

1. pH of the mass during extraction of the pectin content.

2. Time of boil. V. c 3. Size of fibrous cellulose particle.

4.-Quantity of diatomaceous earth present in the mixture.

5. Proportion of pectous bearing materials and 8. Percent of extraction of pectin. It will be appreciated that our products are different from the product of the- Herbert 'r.

Leo Patent No. 1,838,949 in that the fibrous cellulose particles are not ground to colloidal size nor is the pectin present in a water soluble form. Rather instead, the fibrous content of our prod uct is of a suificient size to render filtration roletlvely simple and of accomplishment when a filter aid, ,such as diatomaceous earth, is used. In our product, the potentially available pectin is pment in the form of water inaolublepectose, which, upon subsequent hydrolysis in an acid 50 digestion, is converted into water soluble pectin.

If desired, some of the diatomaceous earth may be removed from the dried product before standardization by grinding and sifting the material through-a screen over 40 mesh, and preferably from am 100 mesh.-. The earth material can then be used over and over again, as it loses none of its properties,- By removing most of this earth material, it is possible to standardize the product and save subsequefit freight charges on this exv vcntion, and we therefore do not purpose 7 the patent granted hereon otherwise than is ncessitated by the prior art. 4 We claim as our invention:

- l. The process of preparing a pectous product which comprises finely grinding fruit pomace to a size greater than colloidal size, washing the ground mass to remove water soluble materials therefrom, saidwashin'g operation being efiected at lowtemperatures to prevent enzymic action, adding a filter aid to the washed mass, pressing the resulting mixture to remove liquid therefrom, disintegrating the resulting pressed paste, rapid ly drying the disintegrated mass at a temperature sufiiciently, low to prevent complete dehydration of the cellulose tissue therein and standardizing the mass to a product of definite iell strength by regulating the amount of filter aid present there- 2. Theprocessof preparing a pectous productv which comprises pressing pectose containing fruits or vegetables to remove juices and oils therefrom, finely." grinding the'pressed'mass to a size greater than colloidal size, repeatedly washing the ground mass to remove water soluble materials therefrom, said washing operation being effected at low temperatures to prevent enzymic action, adding afilter aid to the washed. mass, pressing the resulting mixtureto remove liquid therefrom, disintegrating the resulting pressed paste, rapidly dryin thedisintegrated ,mass at a temperature sumciently IOWQQO prevent complete dehydration of the cellulose tissue" therein and standardizing the mass by removing some of the filter aid to obtain a product of definite jell strength.

3?. The process of preparing a pectous product which comprises pressing pectose containing fruits or vegetables to remove juices and oils therefrom, finely grinding the pressed mass to a size greaterthan colloidal size, repeatedly washing the ground mass to remove water soluble materials therefrom, said washing operation bey ing effected at low temperatures to Prevent. enzymic action, adding dlatomaceous earth to the washed mass, acidifying the resulting mixture with a weak acid to prevent enzymic action, pressing the mixture to remove as much of the 10 liquid therefrom as possible, disintegratingthe t resultingpressed paste, rapidly drying the disintegrated mass at a temperature sufiiciently low to prevent complete dehydration of the cellulose tissue therein and standardizing the productto 15 a definite jell strength with predetermined amounts of dlatomaceous earth.

4. A pectousproduct comprising a dry powv 'dered mixture of greater than colloidal size comprising fibrous crushed fruit or vegetable cellu- 2'0 lose tissue containing substantially the original 7 content of water insoluble pecto'se substantially free from water soluble substances and bitter components of the original fruit or. vegetable, and a filter aid inan amount sufiicient to stand- 25 ardize the product to a definite jell strength.

. 5'. A dry powdered pectous product of greater than colloidal size and-of standardized jell strength comprising a mixture of diatomaceou's earth and finely comminuted' citrus fruit peel 3o containing substantially its original pectose content but substantially free from water soluble substances and bitter components of the origimil citrus fruit peel.

CLARENCE C. TAYLOR. 3 FREDERICK A. BECK. HERBERT T. LEO. 

